CN101935591A - Refinement and extraction method of patchouli oil - Google Patents
Refinement and extraction method of patchouli oil Download PDFInfo
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- CN101935591A CN101935591A CN 201010277844 CN201010277844A CN101935591A CN 101935591 A CN101935591 A CN 101935591A CN 201010277844 CN201010277844 CN 201010277844 CN 201010277844 A CN201010277844 A CN 201010277844A CN 101935591 A CN101935591 A CN 101935591A
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- patchouli oil
- extraction
- ethyl acetate
- phlegma
- patchouli
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Abstract
The invention relates to a technology for extracting volatile oil from patchouli, in particular to a refinement and extraction method of patchouli oil. The method mainly comprises the following three steps: (1) steam distillation; (2) extraction of petroleum ether, ethyl ether and ethyl acetate; and (3) reflux extraction at 55-80 DEG C and 20-40Pa, and collection of condensate of the refined patchouli oil. In the method, patchouli alcohol (C15H26O) content in the obtained condensate of the refined patchouli oil is not less than 26.0%; and by adopting various organic extracts, higher yield up to about 4.2-6.5% can be obtained through calculation of weight of patchouli leaves on the premise of guaranteeing the patchouli alcohol content.
Description
Technical field
The present invention relates to a kind of technology of extracting volatile oil from Wrinkled Gianthyssop Herb, particularly a kind of patchouli oil is made with extra care extracting method.
Background technology
Meet the Patehouli aleohal (C in the patchouli oil that new Chinese Pharmacopoeia requires
15H
26O) content must not be less than 26.0%.Traditional method still is a steam distillation, just uses the decocting liquid of the Wrinkled Gianthyssop Herb in the hot steam-heated cal(l)andria container, regathers the evaporable phlegma, and phlegma is exactly the patchouli oil of slightly carrying.But the Patehouli aleohal in the phlegma of slightly carrying of Shou Jiing has only about 12-18% usually like this, can not reach the requirement of Chinese Pharmacopoeia requirement.Need further refining.
The purified method can be a molecular distillation technique.Supercritical CO
2Technology.It also can be conventional technique of backflow.But produce in the process of patchouli oil in refining industrialization, need take into full account the cost problem of facility investment and technology.Select suitable manner to obtain product.May there be significant difference in the technology of the lab scale of the laboratory stage of refining industrialization and other bibliographical informations.
Summary of the invention
The object of the present invention is to provide a kind of patchouli oil to make with extra care extracting method.
The factor that the present invention considered in the design phase has following:
Must satisfy Patehouli aleohal (C in the patchouli oil end product that obtains
15H
26O) content must not be less than 26.0% requirement.Extract as far as possible and obtain more patchouli oil.Consider the technology that saves production cost.
The technical scheme that we adopt relates generally to three big steps: (1) wet distillation; (2) petroleum ether extraction, extracted with diethyl ether, ethyl acetate extraction; (3) underpressure distillation.
Technical scheme of the present invention is:
Patchouli oil is made with extra care extracting method, wherein:
(1) leaf of Wrinkled Gianthyssop Herb is placed in the inner chamber of container of strap clamp cover, adds the flooding of 5-10 times of weight, and heat steam leads in the chuck and container intracavity simultaneously, collects the phlegma of the patchouli oil that evaporable slightly carries;
The phlegma of the patchouli oil of (2) slightly carrying adds the petroleum ether extraction of 1-3 times of weight, collect the petroleum ether extraction phase, residue is added to the extracted with diethyl ether of 1-3 times of weight, collects the extracted with diethyl ether phase, residue is added to the ethyl acetate extraction of 1-3 times of weight, collects the ethyl acetate extraction phase; Petroleum ether extraction gone up mutually collect residual solution A behind the water distilling apparatus heating recovery sherwood oil, collect residual solution B after extracted with diethyl ether is gone up water distilling apparatus heating recovery ether mutually, will collection residual solution C behind the water distilling apparatus heating recovery ethyl acetate on the ethyl acetate extraction phase;
(3) residual solution A, B, C are merged the back at 55-80 ℃, refluxing extraction under the condition of 20-40Pa, the phlegma of collection purified patchouli oil.
Patehouli aleohal (C in the phlegma of the purified patchouli oil that obtains
15H
26O) content is no less than 26.0%, and because adopted multiple organic extract liquid, under the prerequisite of guaranteeing Patehouli aleohal content, can obtain more productive rate, press the leaf weight calculating of Wrinkled Gianthyssop Herb, productive rate up to 4.2-6.5% about.
If in cancellation sherwood oil, ether, the ethyl acetate extraction liquid any two, Patehouli aleohal (C
15H
26O) content be no less than 26.0% and productive rate be difficult to satisfy simultaneously up to the target of 4.2-7.2%.
The mensuration of Patehouli aleohal is undertaken by the content measuring standard of Chinese Pharmacopoeia in the patchouli oil.
In the existing laboratory lab scale technology that we understand, the content of Patehouli aleohal can be up to 40% in the patchouli oil, but its productive rate is usually about 2%, and this competitive power aspect in extensive industrialization is far to fail in Patehouli aleohal (C of the present invention
15H
26O) content be no less than 26.0% and productive rate up to the combined effect of 4.2-7.2%.
Prior art can adopt that pressurization is refining also can adopt the refining purification patchouli oil of decompression, but the characteristic of maximum of the present invention has found complete technical scheme to guarantee Patehouli aleohal (C still in suitability for industrialized production
15H
26O) content be no less than 26.0% and productive rate up to the combined effect of 4.2-7.2%.
Embodiment
Embodiment 1, the refining extracting method of patchouli oil, wherein:
(1) leaf of Wrinkled Gianthyssop Herb is placed in the inner chamber of container of strap clamp cover, adds the flooding of 5-10 times of weight, and heat steam leads in the chuck and container intracavity simultaneously, collects the phlegma of the patchouli oil that evaporable slightly carries;
The phlegma of the patchouli oil of (2) slightly carrying adds the petroleum ether extraction of 1-3 times of weight, collect the petroleum ether extraction phase, residue is added to the extracted with diethyl ether of 1-3 times of weight, collects the extracted with diethyl ether phase, residue is added to the ethyl acetate extraction of 1-3 times of weight, collects the ethyl acetate extraction phase; Petroleum ether extraction gone up mutually collect residual solution A behind the water distilling apparatus heating recovery sherwood oil, collect residual solution B after extracted with diethyl ether is gone up water distilling apparatus heating recovery ether mutually, will collection residual solution C behind the water distilling apparatus heating recovery ethyl acetate on the ethyl acetate extraction phase;
(3) residual solution A, B, C are merged the back at 55-80 ℃, refluxing extraction under the condition of 20-40Pa, the phlegma of collection purified patchouli oil.
Embodiment 2, the refining extracting method of patchouli oil, wherein:
(1) leaf of Wrinkled Gianthyssop Herb is placed in the inner chamber of container of strap clamp cover, adds the flooding of 5 times of weight, and heat steam leads in the chuck and container intracavity simultaneously, collects the phlegma of the patchouli oil that evaporable slightly carries;
The phlegma of the patchouli oil of (2) slightly carrying adds the petroleum ether extraction of 1 times of weight, collects the petroleum ether extraction phase, and residue is added to the extracted with diethyl ether of 1 times of weight, collects the extracted with diethyl ether phase, and residue is added to the ethyl acetate extraction of 1 times of weight, collects the ethyl acetate extraction phase; Petroleum ether extraction gone up mutually collect residual solution A behind the water distilling apparatus heating recovery sherwood oil, collect residual solution B after extracted with diethyl ether is gone up water distilling apparatus heating recovery ether mutually, will collection residual solution C behind the water distilling apparatus heating recovery ethyl acetate on the ethyl acetate extraction phase;
(3) residual solution A, B, C are merged the back at 55 ℃, refluxing extraction under the condition of 40Pa, the phlegma of collection purified patchouli oil.
Embodiment 3, the refining extracting method of patchouli oil, wherein:
(1) leaf of Wrinkled Gianthyssop Herb is placed in the inner chamber of container of strap clamp cover, adds the flooding of 10 times of weight, and heat steam leads in the chuck and container intracavity simultaneously, collects the phlegma of the patchouli oil that evaporable slightly carries;
The phlegma of the patchouli oil of (2) slightly carrying adds the petroleum ether extraction of 3 times of weight, collects the petroleum ether extraction phase, and residue is added to the extracted with diethyl ether of 3 times of weight, collects the extracted with diethyl ether phase, and residue is added to the ethyl acetate extraction of 3 times of weight, collects the ethyl acetate extraction phase; Petroleum ether extraction gone up mutually collect residual solution A behind the water distilling apparatus heating recovery sherwood oil, collect residual solution B after extracted with diethyl ether is gone up water distilling apparatus heating recovery ether mutually, will collection residual solution C behind the water distilling apparatus heating recovery ethyl acetate on the ethyl acetate extraction phase;
(3) residual solution A, B, C are merged the back at 80 ℃, refluxing extraction under the condition of 20Pa, the phlegma of collection purified patchouli oil.
Embodiment 4, the refining extracting method of patchouli oil, wherein:
(1) leaf of Wrinkled Gianthyssop Herb is placed in the inner chamber of container of strap clamp cover, adds the flooding of 8 times of weight, and heat steam leads in the chuck and container intracavity simultaneously, collects the phlegma of the patchouli oil that evaporable slightly carries;
The phlegma of the patchouli oil of (2) slightly carrying adds the petroleum ether extraction of 2 times of weight, collects the petroleum ether extraction phase, and residue is added to the extracted with diethyl ether of 2 times of weight, collects the extracted with diethyl ether phase, and residue is added to the ethyl acetate extraction of 2 times of weight, collects the ethyl acetate extraction phase; Petroleum ether extraction gone up mutually collect residual solution A behind the water distilling apparatus heating recovery sherwood oil, collect residual solution B after extracted with diethyl ether is gone up water distilling apparatus heating recovery ether mutually, will collection residual solution C behind the water distilling apparatus heating recovery ethyl acetate on the ethyl acetate extraction phase;
(3) residual solution A, B, C are merged the back at 60 ℃, refluxing extraction under the condition of 30Pa, the phlegma of collection purified patchouli oil.
Embodiment 5, the refining extracting method of patchouli oil, wherein:
(3) residual solution A, B, C are merged the back at 55 ℃, refluxing extraction is one hour under the condition of 20Pa, collects the phlegma D of purified patchouli oil; At 60 ℃, refluxing extraction is one hour under the condition of 25Pa, collects the phlegma E of purified patchouli oil; At 70 ℃, refluxing extraction is one hour under the condition of 30Pa, collects the phlegma F of purified patchouli oil.All the other are with embodiment 4.
Embodiment 6, the refining extracting method of patchouli oil, wherein:
(3) residual solution A, B, C are merged the back at 55 ℃, refluxing extraction is one hour under the condition of 30Pa, collects the phlegma D of purified patchouli oil; At 70 ℃, refluxing extraction is one hour under the condition of 30Pa, collects the phlegma E of purified patchouli oil; At 75 ℃, refluxing extraction is one hour under the condition of 40Pa, collects the phlegma F of purified patchouli oil.All the other are with embodiment 3.
Embodiment 7, the refining extracting method of patchouli oil, wherein:
(3) residual solution A, B, C are merged the back at 55 ℃, refluxing extraction is one hour under the condition of 50Pa, collects the phlegma D of purified patchouli oil; At 60 ℃, refluxing extraction is one hour under the condition of 40Pa, collects the phlegma E of purified patchouli oil; At 65 ℃, refluxing extraction is one hour under the condition of 30Pa, collects the phlegma F of purified patchouli oil.All the other are with embodiment 3.
Claims (2)
1. the refining extracting method of patchouli oil is characterized in that: adopt the following step to extract (1) wet distillation; (2) petroleum ether extraction, extracted with diethyl ether, ethyl acetate extraction; (3) underpressure distillation.
2. patchouli oil is made with extra care extracting method, it is characterized in that:
(1) leaf of Wrinkled Gianthyssop Herb is placed in the inner chamber of container of strap clamp cover, adds the flooding of 5-10 times of weight, and heat steam leads in the chuck and container intracavity simultaneously, collects the phlegma of the patchouli oil that evaporable slightly carries;
The phlegma of the patchouli oil of (2) slightly carrying adds the petroleum ether extraction of 1-3 times of weight, collect the petroleum ether extraction phase, residue is added to the extracted with diethyl ether of 1-3 times of weight, collects the extracted with diethyl ether phase, residue is added to the ethyl acetate extraction of 1-3 times of weight, collects the ethyl acetate extraction phase; Petroleum ether extraction gone up mutually collect residual solution A behind the water distilling apparatus heating recovery sherwood oil, collect residual solution B after extracted with diethyl ether is gone up water distilling apparatus heating recovery ether mutually, will collection residual solution C behind the water distilling apparatus heating recovery ethyl acetate on the ethyl acetate extraction phase;
(3) residual solution A, B, C are merged the back at 55-80 ℃, refluxing extraction under the condition of 20-40Pa, the phlegma of collection purified patchouli oil.
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| CN2010102778442A CN101935591B (en) | 2010-09-10 | 2010-09-10 | Refined extraction method of patchouli oil |
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| CN2010102778442A CN101935591B (en) | 2010-09-10 | 2010-09-10 | Refined extraction method of patchouli oil |
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| CN101935591A true CN101935591A (en) | 2011-01-05 |
| CN101935591B CN101935591B (en) | 2012-05-23 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820202A (en) * | 2012-11-16 | 2014-05-28 | 丰益(上海)生物技术研发中心有限公司 | Method for producing fresh zanthoxylum oil |
| CN104208141A (en) * | 2014-09-19 | 2014-12-17 | 成都中医药大学 | New application of patchouli oil in aspect of resisting prostate cancer |
| CN106244328A (en) * | 2016-08-26 | 2016-12-21 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of Herba Pogostemonis essential oil |
| CN107897357A (en) * | 2017-11-23 | 2018-04-13 | 荔浦县万家兴果蔬专业合作社 | A kind of Siraitia grosvenori preservative and its preservation method |
| CN115572641A (en) * | 2022-11-15 | 2023-01-06 | 江西安邦药业有限公司 | Refining and extracting method of patchouli oil |
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| EP0409089B1 (en) * | 1989-07-20 | 1994-12-14 | Kao Corporation | Fragrant patchouli oil and a perfume composition comprising said patchouli oil |
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2010
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Patent Citations (3)
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| EP0409089B1 (en) * | 1989-07-20 | 1994-12-14 | Kao Corporation | Fragrant patchouli oil and a perfume composition comprising said patchouli oil |
| CN101285021A (en) * | 2008-06-06 | 2008-10-15 | 江南大学 | Process for simultaneously abstracting essential oil, chromocor and triterpenes components from agastache |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820202A (en) * | 2012-11-16 | 2014-05-28 | 丰益(上海)生物技术研发中心有限公司 | Method for producing fresh zanthoxylum oil |
| CN104208141A (en) * | 2014-09-19 | 2014-12-17 | 成都中医药大学 | New application of patchouli oil in aspect of resisting prostate cancer |
| CN106244328A (en) * | 2016-08-26 | 2016-12-21 | 广西灏源盛世生物科技有限公司 | A kind of extracting method of Herba Pogostemonis essential oil |
| CN107897357A (en) * | 2017-11-23 | 2018-04-13 | 荔浦县万家兴果蔬专业合作社 | A kind of Siraitia grosvenori preservative and its preservation method |
| CN115572641A (en) * | 2022-11-15 | 2023-01-06 | 江西安邦药业有限公司 | Refining and extracting method of patchouli oil |
| CN115572641B (en) * | 2022-11-15 | 2023-12-19 | 江西安邦药业有限公司 | Refined extraction method of patchouli oil |
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| CN101935591B (en) | 2012-05-23 |
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